Deodorant compositions

ABSTRACT

A deodorant stick comprising: at least about 25% of a liquid triglyceride; at least one antimicrobial; a primary structurant with a melting point of at least about 50° C.; and less than 8% of secondary structurants having a melting point of at least about 60° C.; said stick being free of an aluminum salt; and said stick having a hardness from about 80 mm*10 to about 140 mm*10, as measured by penetration with ASTM D-1321 needle.

CROSS REFERENCE TO RELATED APPLICATIONS

This application claims the benefit of U.S. Provisional Application No.62/527,180, filed Jun. 30, 2017, and of U.S. Provisional Application No.62/647,104, filed Mar. 23, 2018.

FIELD OF THE INVENTION

The present disclosure relates to deodorant compositions and methodsrelating thereto.

BACKGROUND OF THE INVENTION

Many consumers are seeking more natural, aluminum-free deodorantofferings, often mostly free of silicones. Consumers also want a goodglide, non-sticky, and non-greasy application. This is a challenge,because a mostly silicone-free formula will often use natural oils ornatural oil-based triglycerides. But often natural oils, such as coconutoil, bring a large portion of wax with them, often making the resultingdeodorant sticks too hard to meet a more preferable product applicationfor both shaven and unshaven underarms. They are also often undesirablygreasy due to the non-volatile nature.

Thus there remains a challenge to formulate an aluminum-free, mostlysilicone-free deodorant stick that is not too hard.

SUMMARY OF THE INVENTION

A deodorant stick comprising: at least about 25% of a liquidtriglyceride; at least one antimicrobial; a primary structurant with amelting point at least about 50° C.; and less than 8% of secondarystructurants having a melting point of at least about 60° C.; said stickbeing free of an aluminum salt; and said stick having a hardness fromabout 80 mm*10 to about 140 mm*10, as measured by penetration with ASTMD-1321 needle.

DETAILED DESCRIPTION OF THE INVENTION

While the specification concludes with claims that particularly pointout and distinctly claim the invention, it is believed the presentinvention will be better understood from the following description.

The present invention can comprise, consist of, or consist essentiallyof the essential elements and limitations of the invention describedherein, as well any of the additional or optional ingredients,components, or limitations described herein.

All percentages, parts and ratios are based upon the total weight of thecompositions of the present invention, unless otherwise specified. Allsuch weights as they pertain to listed ingredients are based on theactive level and, therefore do not include carriers or by-products thatmay be included in commercially available materials.

The components and/or steps, including those which may optionally beadded, of the various embodiments of the present invention, aredescribed in detail below.

All documents cited are, in relevant part, incorporated herein byreference; the citation of any document is not to be construed as anadmission that it is prior art with respect to the present invention.

All ratios are weight ratios unless specifically stated otherwise.

All temperatures are in degrees Celsius, unless specifically statedotherwise.

Except as otherwise noted, all amounts including quantities,percentages, portions, and proportions, are understood to be modified bythe word “about”, and amounts are not intended to indicate significantdigits.

Except as otherwise noted, the articles “a”, “an”, and “the” mean “oneor more”.

Herein, “comprising” means that other steps and other ingredients whichdo not affect the end result can be added. This term encompasses theterms “consisting of” and “consisting essentially of”. The compositionsand methods/processes of the present invention can comprise, consist of,and consist essentially of the essential elements and limitations of theinvention described herein, as well as any of the additional or optionalingredients, components, steps, or limitations described herein.

Herein, “effective” means an amount of a subject active high enough toprovide a significant positive modification of the condition to betreated. An effective amount of the subject active will vary with theparticular condition being treated, the severity of the condition, theduration of the treatment, the nature of concurrent treatment, and likefactors.

The term “anhydrous” as used herein means substantially free of added orfree water. From a formulation standpoint, this means that the anhydrousdeodorant stick compositions of the present invention contain less thanabout 1%, and more specifically zero percent, by weight of free or addedwater, other than the water of hydration typically associated with theparticulate deodorant active prior to formulation.

The term “ambient conditions” as used herein refers to surroundingconditions under about one atmosphere of pressure, at about 50% relativehumidity, and at about 25° C., unless otherwise specified. All values,amounts, and measurements described herein are obtained under ambientconditions unless otherwise specified.

The term “majority” refers to greater than about 51% of the statedcomponent or parameter.

“Substantially free of” refers to about 2% or less, about 1% or less, orabout 0.1% or less of a stated ingredient. “Free of” refers to nodetectable amount of the stated ingredient or thing.

The term “volatile” as used herein refers to those materials that have ameasurable vapor pressure at 25° C. Such vapor pressures typically rangefrom about 0.01 millimeters of Mercury (mm Hg) to about 6 mmHg, moretypically from about 0.02 mmHg to about 1.5 mmHg; and have an averageboiling point at one (1) atmosphere of pressure of less than about 250°C., more typically less than about 235° C. Conversely, the term“non-volatile” refers to those materials that are not “volatile” asdefined herein.

As consumers seek more natural ingredients in their deodorants, oneapproach to formulation is to use emollients derived from natural oils.Emollients derived from natural oils are derived from plant sources,such as palm oil or coconut oil. One example of an emollient derivedfrom natural oils may be a liquid triglyceride, defined as liquid at 25°C. Thus, products that hope to emphasize natural ingredients may have asignificant amount of a liquid triglyceride, for example.

In order to provide structure to the deodorant stick composition, theformulation may also include a number of waxes and other structurants.However, the structurants used may lead to deodorant sticks that arevery hard. For example, a currently marketed product, ComparativeFormula 1 below, has 34.15% liquid triglyceride, along with a number ofstructurants, resulting in a very hard stick, scoring 63 on a needlepenetration test under ASTM D-1321 (as described herein). So whileComparative Formula 1 uses consumer-preferred natural ingredients, itdoes not necessarily provide a good consumer experience when used, givenits hardness. Comparative Formula 2 contains even higher levels ofstructurants, resulting in a harder stick with an even lower hardnessscore. In comparison, Inventive Examples 1-5, while comprisingconsumer-preferred natural ingredients, have higher hardness scores,meaning they are softer products.

TABLE 1 Comparative Comparative Inventive Inventive Inventive InventiveInventive Formula Formula Example Example Example Example Example 1 2 12 3 4 5 Hardness 63 56 97 90 117 86 85 (Penetration mm*10) Caprylic/34.15 31.15 43.4 44.7 42.7 46.9 46.15 Capric Triglyceride Arrowroot 2323 19 23 23 19 Powder Stearyl 12 12 11.5 10.7 10.7 Alcohol Ozokerite 1.511 11.75 Castor 3 4 3 3 3 Wax Baking 12 12 12 12 6 6 Soda Magnesium 6 612.0 Hydroxide Shea Butter 6 6 2 2 2 2 2 Coconut 4.75 4.75 4.5 4.5 4.54.5 4.5 Oil Poly- 2.5 3.5 glycerol-3 Beeswax Jojoba 1 2 Esters 70Glyceryl 1 1 Caprylate (and) Glyceryl Undecylenate Perfumes 0.6 0.6 0.60.6 0.6 0.6 0.6 Cyclo- 4 4 4 dextrin Tapioca 19.0 Starch

It is known that to formulate a solid antiperspirant or deodorant stick,the structurants generally have a melting point above 50° C. to providea stable structure to the stick. The present inventors have discoveredthat a deodorant stick having at least about 25% of a liquidtriglyceride, and that uses a primary structurant that has a meltingpoint of at least about 50° C., in some embodiments from about 50° C. to70° C. and in still other embodiments from about 50° C. to about 75° C.,while limiting the amount of secondary structurants having a meltingpoint of at least about 60° C. to 8% or less, can result in a deodorantstick with a hardness from about 80 mm*10 to about 140 mm*10. Such adeodorant stick is able to comprise consumer-perceived naturalingredients, while offering a pleasant consumer experience in terms ofits hardness.

A. Structurants

The deodorant compositions of the present invention comprise a suitableconcentration of structurants to help provide the compositions with thedesired viscosity, rheology, texture and/or product hardness, or tootherwise help suspend any dispersed solids or liquids within thecomposition.

The primary structurant in the present invention may have a meltingpoint of at least about 50° C., in some embodiments from about 50° C. toabout 70° C., and in other embodiments from about 50° C. to about 75°C., and in other embodiments from about 60° C. to 80° C. A primarystructurant is defined as the structurant that is present in thecomposition in the greatest amount (liquid triglycerides are notconsidered a structurant in this context). Some embodiments may havejust a single structurant, so may have only a primary structurant. Otherembodiments may have a primary structurant and then secondarystructurants, those structurants that are used in a lesser amount thanthe primary structurant.

The primary structurant may comprise from about 5% to about 20%, in somecases 7-17% of the deodorant stick. The secondary structurants maycumulatively comprise about 12% or less, or about 8% or less of thedeodorant stick, in some embodiments less than about 5%, less than about3%, or less than about 1% of the deodorant stick. In some embodiments,the deodorant stick may be free of or substantially free of anysecondary structurants

In some embodiments, some secondary structurants may have a meltingpoint less than 60° C., and then remaining secondary structurants have amelting point of at least about 60° C. The percentage of secondarystructurants having a melting point less than 60° C. may not be assignificant as the percentage of secondary structurants having a meltingpoint of at least about 60° C., as the higher melting structurants arewhat contribute more to the hardness of the deodorant stick. So in someembodiments, the secondary structurants having a melting point of atleast about 60° C. may cumulatively comprise 8% or less of the deodorantstick, in some embodiments less than about 5% of the deodorant stick,less than about 3% of the deodorant stick, or less than about 1% of thedeodorant stick. In some embodiments, the deodorant stick may be free ofor substantially free of any secondary structurants having a meltingpoint of at least about 60° C.

The term “structurant” as used herein means any material known orotherwise effective in providing suspending, gelling, viscosifying,solidifying, and/or thickening properties to the composition or whichotherwise provide structure to the final product form.

Waxes with melting points between 50° C. and 70° C. include Japan wax,lemon wax, grapefruit wax, beeswax, ceresine, paraffin, hydrogenatedjojoba, ethylene glycol distearate, stearyl stearate, palmityl stearate,stearyl behenate, cetearyl behenate, hydrogenated high erucic acidrapeseed oil, and stearyl alcohol.

Waxes with melting points above 70° C. include ozokerite, candelilla,carnauba, espartograss, cork wax, guaruma, rice oil wax, sugar cane wax,ouricury, montan ester wax, sunflower wax, shellac, ozocerite,microcrystalline wax, sasol wax, polyethylenes, polymethylenes, ethyleneglycol dipalmitate, ethylene glycol di(12-hydroxystearate), behenylbehenate, glyceryl tribehenate, hydrogenated castor oil (castor wax),and behenyl alcohol.

Waxes with melting points that could vary and possibly fall into eitherof the two previous groups (depending on factors such as chain length)include C18-C36 triglyceride, Fischer-Tropsch waxes, silicone waxes,C30-50 alkyl beeswax, C20-40 alkyl erucates, C18-38 alkyl hydroxystearoyl stearates, C20-40 dialkyl esters of dimer acids, C16-40 alkylstearates, C20-40 alkyl stearates, cetyl ester wax, and spermaceti.

Suitable gelling agents include fatty acid gellants such as fatty acidand hydroxyl or alpha hydroxyl fatty acids, having from about 10 toabout 40 carbon atoms, and ester and amides of such gelling agents.Non-limiting examples of such gelling agents include, but are notlimited to, 12-hydroxystearic acid, 12-hydroxylauric acid,16-hydroxyhexadecanoic acid, behenic acid, eurcic acid, stearic acid,caprylic acid, lauric acid, isostearic acid, and combinations thereof.Preferred gelling agents are 12-hydroxystearic acid, esters of12-hydroxystearic acid, amides of 12-hydroxystearic acid andcombinations thereof.

These solid structurants include gelling agents, and polymeric ornon-polymeric or inorganic thickening or viscosifying agents. Suchmaterials will typically be solids under ambient conditions and includeorganic solids, crystalline or other gellants, inorganic particulatessuch as clays or silicas, or combinations thereof.

The concentration and type of solid structurant selected for use in thedeodorant compositions will vary depending upon the desired producthardness, rheology, and/or other related product characteristics. Formost structurants suitable for use herein, the total structurantconcentration ranges from about 5% to about 35%, more typically fromabout 10% to about 30%, or from about 7% to about 20%, by weight of thecomposition.

Non-limiting examples of suitable primary structurants include stearylalcohol and other fatty alcohols; hydrogenated castor wax (e.g.,Castorwax MP80, Castor Wax, etc.); hydrocarbon waxes include paraffinwax, beeswax, carnauba, candelilla, spermaceti wax, ozokerite, ceresin,baysberry, synthetic waxes such as Fisher-Tropsch waxes, andmicrocrystalline wax; polyethylenes with molecular weight of 200 to 1000daltons; solid triglycerides; behenyl alcohol, or combinations thereof.The deodorant stick may further comprise one or more structural elementsselected from the group consisting of waxes, natural oils, coconut oil,fractionated coconut oil, jojoba seed oil, olive oil, soybean oil,sunflower oil, and combinations thereof.

Other non-limiting examples of primary structurants suitable for useherein are described in U.S. Pat. No. 5,976,514 (Guskey et al.) and U.S.Pat. No. 5,891,424 (Bretzler et al.), the descriptions of which areincorporated herein by reference.

Non-limiting examples of suitable additional structurants includestearyl alcohol and other fatty alcohols; hydrogenated castor wax (e.g.,Castorwax MP80, Castor Wax, etc.); hydrocarbon waxes include paraffinwax, beeswax, carnauba, candelilla, spermaceti wax, ozokerite, ceresin,baysberry, synthetic waxes such as Fisher-Tropsch waxes, andmicrocrystalline wax; polyethylenes with molecular weight of 200 to 1000daltons; and solid triglycerides; behenyl alcohol, or combinationsthereof.

Other non-limiting examples of additional structurants suitable for useherein are described in U.S. Pat. No. 5,976,514 (Guskey et al.) and U.S.Pat. No. 5,891,424 (Bretzler et al.).

B. Emollients

As discussed, an effective and consumer-preferred emollient may be aliquid triglyceride. Derived directly from plant sources, they are oftenshort chains. Longer chain triglycerides may be used as structurants indeodorant or antiperspirant sticks, but the triglycerides of the presentinvention are liquid at room temperature (25° C.) and tend to be shorterchains. An example may be caprylic/capric triglyceride (coconut oilfractionated).

The present inventive deodorant sticks may comprise at least about 25%of one or more liquid triglyceride, in some embodiments, at least about30%, at least 35%, at least about 40%, at least about 45%, or at leastabout 50% liquid triglyceride, by weight of the composition. In someembodiments, the deodorant stick comprises from about 25% to about 60%,by weight of the composition, of one or more liquid triglyceride, fromabout 25% to about 50%, from about 30% to about 50%, from about 35% toabout 60%, from about 35% to about 50%, from about 40% to about 60%, orfrom about 40% to about 50%, by weight of the composition, of one ormore liquid triglyceride. In general, the greater amount of liquid inthe formulation, the softer the deodorant stick may be. The more solidsin the formulation leads to greater hardness. Because achieving asufficient softness in a deodorant stick with natural ingredients can bea challenge, it can be beneficial to formulate with higher amounts ofliquids such as liquid triglyceride. The level of liquid triglyceride asreferred to herein may be the sum total of one or more types of liquidtriglyceride in a particular deodorant stick.

In some embodiments, additional emollients may be used, such as plantoils (generally used at less than 10%) including olive oil, coconut oil,sunflower seed oil, jojoba seed oil, avocado oil, canola oil, and cornoil. Additional emollients including mineral oil; shea butter, PPG-14butyl ether; isopropyl myristate; petrolatum; butyl stearate; cetyloctanoate; butyl myristate; myristyl myristate; C12-15 alkylbenzoate(e.g., Finsolv™); octyldodecanol; isostearyl isostearate; octododecylbenzoate; isostearyl lactate; isostearyl palmitate; isobutyl stearate;dimethicone, and any mixtures thereof.

C. Antimicrobials

The present invention may include one or more antimicrobialcompositions. For example, antimicrobials may include, without beinglimited to, baking soda, hexamidine, magnesium carbonate, zinccarbonate, thymol, magnesium hydroxide, magnesium hydroxide andmagnesium carbonate hydroxide (dead sea salt), partially carbonatedmagnesium hydroxide, sodium carbonate, calcium carbonate, magnesiumcarbonate hydroxide, cinnamon essential oil, cinnamon bark essentialoil, cinnamic aldehyde, polyvinyl formate, salycilic acid, niacinamide,phenoxyethanol, eugenol, linolenic acid, dimethyl succinate, citral,triethyl citrate, sepiwhite, an substituted or unsubstituted2-pyridinol-N-oxide material (piroctone olamine), and combinationsthereof. The deodorant stick may be free of or substantially free of asubstituted or unsubstituted 2-pyridinol-N-oxide material.

In general, the total amount of antimicrobial used in the presentinvention may be from about 0.1% to about 30%, by weight, of thedeodorant. Some antimicrobials may be used in amounts as low as about0.1%, by weight of the deodorant stick, such as if using piroctoneolamine or hexamidine as the primary antimicrobial, while others couldbe as high as about 25% if using magnesium hydroxide or magnesiumhydroxide and magnesium carbonate hydroxide as the primary antimicrobial(primary antimicrobial being the antimicrobial present in thecomposition in the highest amount). In the latter cases, baking sodamight still be used at a lower level, such as from about 0.1% to about6%, as a secondary antimicrobial, or not at all.

Any of the antimicrobials of the present invention may be used aspowders. It is believed that antimicrobial powders may provide a betterdeposition and have more longevity on the skin than antimicrobialsdelivered in a different form. In addition, it is believed thatantimicrobial powders of a certain average particle size, typically fromabout 1 micron to about 5 microns, may provide a significant increase inantimicrobial efficacy.

Many antimicrobials can be effective at minimizing the skin surfacebacteria. However, as a leave-on product where odor may not occur untillater, even hours after application, deodorant antimicrobials are neededthat will be effective for long periods of time. So while deodorantantimicrobials may be effective immediately upon application on theskin, it is believed that odor comes back quickly because the bacterialiving around the hair follicle can quickly repopulate the skin surfacebacteria. Historical approaches using high skin penetrating liquidantimicrobials to affect this region (for example, hexanediol) can causeirritation. Therefore, the present invention may target methods andmechanisms that can more effectively deliver antimicrobials not only tothe skin surface, but to the bacteria in and around the hair follicle.While not wanting to be bound to the theory, the inventors of thepresent inventor believe that powders, specifically powders with anaverage particle size of less than about 10 microns, in some cases fromabout 1 micron to about 5 microns, are more efficient at getting intothe hair follicle where the bacteria live and repopulate the skinsurface. In some embodiments, the antimicrobials may be a combination oflarger sized particles and smaller particles that are from 1 to 10microns. As noted above, solids such as powders can impact the overallhardness of the deodorant stick. In general, greater amounts of powdersand structurants increase the deodorant stick's hardness.

The present inventors have discovered that the water solubilities ofcertain components in the solid stick deodorant have great importance.Some deodorant ingredients will bring in moisture to the batch, whichcan solvate these components to different extents when the waterevaporates and subsequently recondenses as free water in the batch.Certain batch processing conditions (such as a closed top on the tank)could more effectively trap this water in the tank, where it is thenfree to interact with components of the batch. For example, highly watersoluble alkaline powders can contribute negatively towards natural andessential oil stability when dissolved. This is because many natural andessential oils contain a broad range of perfume chemicals, many of whichcan undergo degradation reactions when exposed to extreme pH or heat.This is why many natural and essential oils have shorter shelf livesthan many commercial synthetic chemicals or perfumes. And certainantimicrobials may cause irritation due to high water solubility.Further, high water solubility can lead to grittier products as the morewater soluble powders can agglomerate when exposed to moisture releasedfrom powders during the heat of manufacture.

Thus, embodiments of the present invention may include an antimicrobialwith a low water solubility. An antimicrobial with a low watersolubility may be, in some embodiments, an antimicrobial with a watersolubility of at most 90 g/L at 25° C., in other embodiments at most 75g/L at 25° C., or in still other embodiments at most 50 g/L at 25° C.

Materials with a water solubility above 90 g/L @25° C. include but arenot limited to: potassium carbonate, potassium bicarbonate, sodiumcarbonate, sodium sesquicarbonate, triethyl citrate, and baking soda.Materials with a water solubility below 90 g/L @25° C. include but arenot limited to: beryllium carbonate, magnesium carbonate, calciumcarbonate, magnesium hydroxide, magnesium hydroxide and magnesiumcarbonate hydroxide, partially carbonated magnesium hydroxide, piroctoneolamine, hexamidine, zinc carbonate, thymol, polyvinyl formate,salycilic acid, phenoxyethanol, eugenol, linolenic acid, dimethylsuccinate, citral, and triethyl citrate. Each of beryllium carbonate,magnesium carbonate, calcium carbonate, magnesium hydroxide, magnesiumhydroxide and magnesium carbonate hydroxide, partially carbonatedmagnesium hydroxide, piroctone olamine, hexamidine, zinc carbonate,thymol, polyvinyl formate, salycilic acid, phenoxyethanol, eugenol,linolenic acid, dimethyl succinate, and citral have a water solubilitybelow 75 g/L @25° C., below 50 g/L @25° C., below 1 g/L @25° C., andbelow 0.2 g/L @25° C.

D. Antimicrobial Activity

Table 2 below shows the raw material microbial inhibition concentrationdata tested against two key underarm bacteria strains. As can be seen,the first three listed antimicrobials, lupamin, hexamidine, andpiroctone olamine, perform particularly well against the bacteria as rawmaterials. Also performing well as raw materials are phenoxyethanol,eugenol, linolenic acid, dimethyl succinate, citral, triethyl citrate,and sepiwhite. Also performing moderately well against the bacteria asraw materials were magnesium carbonate/magnesium hydroxide and calciumcarbonate.

TABLE 2 Antimicrobial C. mucofaciens S. epidermidis Lupamin <2 ppm 4 ppmHexamidine 36 mg/ml H2O <2 ppm 7 ppm 100 mg/ml piroctone olamine in H2O<5 ppm 10 ppm 100% Phenoxyethanol 400 ppm 800 ppm % Eugenol 99% ETOH 773ppm 773 ppm Linolenic Acid 70% ETOH 1093 ppm 1093 ppm Dimethyl Succinate98% ETOH 1531 ppm 3062 ppm Citral 96% ETOH 1500 ppm 1500 ppm 100%Triethyl citrate 1600 ppm 1600 ppm Sepiwhite 40 mg/ml H2O ins 2000 ppm1000 ppm Magnesium Carbonate & Magnesium >2500 ppm >2500 ppm Hydroxide50 mg/ml H2O ins Ca Carbonate 50 mg/ml H2O ins >2500 ppm >2500 ppmLinoleic acid 100% ETOH 3125 ppm 3125 ppm Conarom B (beta Bio) 100% ETOH3125 ppm 3125 ppm Hexyl Decanol 97% ETOH 6062 ppm 3031 ppm Ajowan oil50% ETOH 12500 ppm 6300 ppm Oregano oil 50% ETOH 12500 ppm 6300 ppm 100%Ethylhexyl glycerin 12500 ppm 12500 ppm Mineral oil 50% in ETOH 12500ppm >50000 ppm ACH 50% in H2O 25000 ppm 25000 ppm NaCl 250 mg/mlH2O >25000 ppm >25000 ppm Farnesol 95% ETOH 47500 ppm 5937 ppm Phytol97% ETOH >49000 ppm >49000 ppm Nerolidol 98% ETOH >49000 ppm >49000 ppmCaCl 500 mg/ml H2O >50000 ppm >50000 ppm Isopropyl Myristate 98%ETOH >59000 ppm >59000 ppm

While numerous antimicrobials exhibit efficacy against two main bacteriastrains that antiperspirants and deodorants try to address, due toregulatory and safety reasons, there are sometimes limits as to how muchof a particular antimicrobial may be put into an antiperspirant ordeodorant formula. Therefore, there may be a need for multipleantimicrobials to work together in a formula to deliver enough long-termodor protection.

Deodorant Composition

The deodorant compositions as described herein can contain astructurant, an antimicrobial, a perfume, and additional chassisingredient(s). The deodorant composition may further comprise otheroptional ingredient(s). The compositions can be in the form of a solidstick. The compositions may be free of dipropylene glycol, added water,castor wax, or any combination thereof. The compositions may besubstantially free of or free of a substituted or unsubstituted2-pyridinol-N-oxide material (piroctone olamine). The deodorantcomposition may be anhydrous. The deodorant composition may be free ofadded water.

Hardness

The deodorant compositions of the present invention may have a productor stick hardness from about 80 mm*10 to about 140 mm*10, as measured bypenetration with ASTM D-1321 needle (see Hardness test method below). Insome embodiments, the product hardness may be from about 80 to about 120mm*10, and in others from about 85 to about 100 mm*10.

Perfume

Perfumes are often a combination of many raw materials, known as perfumeraw materials. Any perfume suitable for use in a deodorant compositionmay be used herein. In some embodiments, the deodorant composition maybe free of, or substantially free of a synthetic fragrance. A syntheticfragrance is one mostly derived through chemical synthesis where thestarting material is no longer intact, but is converted to the newfragrance chemical.

A natural or essential oil fragrance is a result of natural sourceswherein the fragrance material is not altered (chemically modified) butextracted from its natural source. These sources can include, but arenot limited to, bark, flowers, blossoms, fruits, leaves, resins, roots,bulbs, and seeds. Natural or essential oils go through an extractionprocess instead of chemical synthesis. Extraction processes include, butare not limited to, maceration, solvent extraction, distillation,expression of a fruit peel, or effleurage.

Additional Chassis Ingredients

Starch

The deodorant composition may comprise a starch powder for dry feel orwetness absorption. Examples include but are not limited to arrowrootpowder, tapioca starch, and corn starch.

Solvent

Non-Volatile Organic Fluids

Non-volatile organic fluids may be present, for example, in an amount ofabout 15% or less, by weight of the composition.

Non-limiting examples of nonvolatile organic fluids include mineral oil,PPG-14 butyl ether, isopropyl myristate, petrolatum, butyl stearate,cetyl octanoate, butyl myristate, myristyl myristate, C12-15alkylbenzoate (e.g., Finsolv™), octyldodecanol, isostearyl isostearate,octododecyl benzoate, isostearyl lactate, isostearyl palmitate, andisobutyl stearate.

Other Optional Ingredients

The anhydrous deodorant compositions of the present invention mayfurther comprise any optional material that is known for use inantiperspirant and deodorant compositions or other personal careproducts, or which is otherwise suitable for topical application tohuman skin.

One example of an optional ingredient is a scent expression material.Scent expression or release technology may be employed with some or allof the fragrance materials to define a desired scent expression prior touse and during use of the deodorant products. Such scent expression orrelease technology can include cyclodextrin complexing material, likebeta cyclodextrin. Other materials, such as, for example, starch-basedmatrices or microcapsules may be employed to “hold” fragrance materialsprior to exposure to bodily-secretions (e.g., perspiration). Theencapsulating material may have release mechanisms other than via asolvent; for example, the encapsulating material may be frangible, andas such, rupture or fracture with applied shear and/or normal forcesencountered during application and while wearing. A microcapsule may bemade from many materials, one example is polyacrylates.

Another example of optional materials are clay mineral powders such astalc, mica, sericite, silica, magnesium silicate, syntheticfluorphlogopite, calcium silicate, aluminum silicate, bentonite andmontomorillonite; pearl pigments such as alumina, barium sulfate,calcium secondary phosphate, calcium carbonate, titanium oxide, finelydivided titanium oxide, zirconium oxide, zinc oxide, hydroxy apatite,iron oxide, iron titrate, ultramarine blue, Prussian blue, chromiumoxide, chromium hydroxide, cobalt oxide, cobalt titanate, titanium oxidecoated mica; organic powders such as polyester, polyethylene,polystyrene, methyl methacrylate resin, cellulose, 12-nylon, 6-nylon,styrene-acrylic acid copolymers, poly propylene, vinyl chloride polymer,tetrafluoroethylene polymer, boron nitride, fish scale guanine, lakedtar color dyes, laked natural color dyes; and combinations thereof.

Talc, if used at higher levels can produce a significant amount of whiteresidue which has been found to be a consumer negative for productacceptance. Therefore it is best to limit the composition to less than10%, less than about 8%, less than about 6%, or less than about 3%, byweight of the composition.

Nonlimiting examples of other optional materials include emulsifiers,distributing agents, antimicrobials, pharmaceutical or other topicalactive, preservatives, surfactants, chelants, and so forth. Examples ofsuch optional materials are described in U.S. Pat. No. 4,049,792(Elsnau); U.S. Pat. No. 5,019,375 (Tanner et al.); and U.S. Pat. No.5,429,816 (Hofrichter et al.); which descriptions are incorporatedherein by reference.

Method of Making

The deodorant stick products of the present invention may be made bymixing all the components of the products in an open-top or vented tank.Many powders come with bound moisture, especially naturally highmoisture powders like starches. In a mostly anhydrous process withwaxes, melting the waxes above their melt point can release this boundwater as the batch temperature increases. In a closed tank process thiswater vapor will condense in the tank and drip back into the batch aswater. This water can interact with the most water soluble ingredientsin the batch to have negative effects on the product, includingreleasing the pH of any antimicrobial ingredient, which can then degradeany perfume ingredients in the batch. Additionally, the condensed watercan interfere with the wax and produce a stick softer than intended.

The present invention reduces the risk of these negative consequences.The ideal process remedy for this behavior is to produce the batches inone of four ways:

-   -   1. An open tank system where the water vapor can leave the batch        tank to reduce or eliminate condensation.    -   2. A vented closed tank to also remove water vapor during the        batch process.    -   3. A dual phase process where the moisture containing powders        can be put into the cold phase separate from the wax phase which        is heated. These two phases are then mixed before filling.    -   4. A low residence time batch process for a closed system, where        the product has less than 3 hours residence time above 50° C. to        reduce the rate of reaction from the moisture.

A method of making a deodorant composition or stick may comprise thesteps of combining any of the herein described deodorant compositioncomponents in an open tank system or a vented closed tank. Thecomponents may be mixed, heated, and then cooled into a stick product.In some embodiments, the deodorant components may comprise at leastabout 40% of a liquid triglyceride, by weight of the composition, and anantimicrobial in an open tank system, heating the components, mixing thecomponents, and cooling the components.

Test Methods

Hardness Test Method—Penetration Measurement for Deodorant FinishedProducts

The penetration test is a physical test method that provides a measureof the firmness of waxy solids and extremely thick creams and pasteswith penetration values not greater than 250 when using a needle forD1321. The method is based on the American Society for Testing andMaterials Methods D-5, D1321 and D217 and DIN 51 579 and is suitable forall solid antiperspirant and deodorant products.

A needle or polished cone of precisely specified dimensions and weightis mounted on the bottom of a vertical rod in the test apparatus. Thesample is prepared as specified in the method and positioned under therod. The apparatus is adjusted so that the point of the needle or coneis just touching the top surface of the sample. Consistent positioningof the rod is critical to the measured penetration value. The rod isthen released and allowed to travel downward, driven only by the weightof the needle (or cone) and the rod. Penetration is the tenths of amillimeter travelled following release.

APPARATUS SUGGESTED TYPE (OR EQUIVALENT) Penetrometer with TimerPenetrometer Suitable For ASTM D-5 and D- (see attached drawings 1321methods; Examples: Precision or Attachment 1 and Humboldt UniversalPenetrometer (Humboldt Attachment 2) Manufacturing, Schiller Park, ILUSA) or Penetrometer Model PNR10 or PNR12 (Petrolab USA or PetroTestGmbH). Penetration Needles ANTIPERSPIRANT or DEODORANT SOLIDS can use:  Needles as specified for ASTM Method   D-5, NIST Certified, FisherScientific   #01-512.   Needles as specified for ASTM Method   D1321/DIN 51 579, Officially certified,   Taper-Tipped needle, No.H-1310,   Humboldt Mfg.General Instructions—All Penetrometers—Keep the instrument andneedles/probes clean at all times, free from dust and grime. When not inuse, store needles in a suitable container to avoid damage. Periodiccalibration should confirm:

Electronic Timer is correctly set. Verify against an independentstopwatch if unsure.

Shaft falls without visible signs of frictional resistance.

Ensure the total weight of the shaft and needle is 50±0.2 grams when theshaft is in free fall. Note: for modern, automated or digital systemsthis may be performed automatically and confirmed through annualcalibration.

At Time of Use Confirm:

Electronic Timer is correctly set to 5.0 seconds.

The appropriate needle is installed and is clean, straight and withoutobvious defects (visual inspection)

The penetrometer is level and the shaft is clean, straight and fallsfreely (visual inspection)

Once level, avoid shifting the position of the unit to maintain level.

Sample Preparation and Measurement

1. On a deodorant stick that has cooled ambiently to a temperaturebetween 22° C. and 26° C. for at least 24 hours, slice off top ½ inch ofproduct to achieve a flat surface with a wire cutter drawn across theupper lip of the canister.2. For the first sample to be tested, lubricate the needle by gentlywiping with a lint-free tissue coated with a small amount of the productto be tested. This small amount is typically taken from the shaved top.3. Place the canister in the appropriate location for the measurement.Locate the sample so the needle will penetrate the product 9-11 mm fromthe inside of the canister wall on the long axis.4. Using the coarse and fine adjustments, align the height of thepenetrometer mechanism head so that the point of the penetrating needleis just touching the surface of the sample.A weak light at the side of the penetrometer which casts a shadow of theneedle on the surface of the sample may be helpful in determining thiscontact. When a light area on the sample cannot be seen at the end ofthe tip of the needle's shadow, the needle height over the sample iscorrectly adjusted. The light should not be strong enough to heat ormelt the sample surface. The needle should be just close enough toscratch the sample surface.5. Perform the penetration measurement at this location by releasing theneedle. Record the result.6. Repeat Steps 2 through 4 at the other test point, i.e., at the otherpoint 9-11 mm inside of the canister wall on the long axis.

To report results, units for penetration are tenths of a millimeter (1/10 mm=100 microns). For example, a result of 80 units is 80 mm*10 or 8mm. Report the average results of at least 4 total measurements from 2different sticks, report to the nearest tenth of a millimeter.

Tier 1 Anaerobic MIC Assay

The data in Table 2 above was generated with the following test method.The purpose of this assay is to determine if a compound or formulationhas an antimicrobial effect in vitro.

It is understood that when not specifically noted in this procedure:

a) All materials, reagents and equipment required for this procedure areof appropriate design and condition of cleanliness and/or sterility asdetermined by their intended use.

b) The operator has been trained in aseptic technique and has beenqualified to perform the procedure and accurately interpret the results.

c) All media required for this procedure was manufactured by a reputablecommercial source egg. Difco, Merck etc. and has been stored andprepared as per manufacturer's instructions.

d) All routine laboratory controls, including but not limited to, mediafunction and growth promotion tests, verification of sterility and useof positive and negative controls are being conducted.

Procedure: (All procedures performed in anaerobic chamber except wherenoted)

1. Apparatus

-   -   Incubator at 37° C.; 20-200 ul 12 channel pipette; 5-50 ul 12        channel pipette; 1250 ul 8 channel Thermo Scientific Matrix        pipette; 96 well plate shaker (located in incubator); Beckman        Coulter deep well cap mat #267005; Beckman Coulter deep 96 well        plates #267007; Falcon 96 well tissue culture plates #353072;        Vortexer; Culture tubes/caps Disposable sterile gloves; Sterile        petri dishes; Standard microbiological lab equipment (sterile        pipettes, syringes, tips, loops, etc.); Glass bottles/flasks for        media; Autoclave;

Parafilm; Spectrophotometer.

2. Media

-   -   0.9% or 0.85% saline solution    -   BHI agar supplemented with 1% Tween 80    -   BHI media supplemented with 1% Tween 80

3. Microbial Strains

-   -   Staphylococcus epidermidis (clinical isolate)    -   Corynebacterium mucofaciens (clinical isolate)

4. Test Procedure

Inoculum Preparation

-   -   Prior to testing streak organisms for isolation on BHI with 1%        Tween 80 plates, wrap with parafilm and place in 37° C.        incubator. When isolated colonies appear remove one        representative colony from each plate and place each in 5 ml of        BHI with 1% Tween 80 media. Incubate at 37° C. with shaking        overnight. Inoculate 20 ml BHI with 1% Tween 80 (per 96 deep        well plate to be tested) with 20 ul of the overnight culture        (1-1000 dilution).

Master Plate Preparation

-   -   Compounds/formulations to be tested are diluted across a 96 deep        well plate as shown below (for a 1% stock solution). 800 ul of        0.85% saline is added to wells A1 and B1 (as these will be the        negative and positive control respectively). 800 ul each 1%        stock solution+positive control are added to wells C1 through        H1. 400 ul 0.85% saline are added to all other wells. 400 ul is        then removed from #1 well added to the #2 well and mixed. This        is then continued across the plate resulting in a 50% dilution        between wells across the plate (this can be easily accomplished        with an automatic 8 channel Matrix pipette set to withdraw,        dispense and mix).

1 2 3 4 5 6 7 8 9 10 11 12 A 800 ul saline 400 ul 400 ul 400 ul 400 ul400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul NaCl NaCl NaCl NaClNaCl NaCl NaCl NaCl NaCl NaCl NaCl B 800 ul saline 400 ul 400 ul 400 ul400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul NaCl NaCl NaClNaCl NaCl NaCl NaCl NaCl NaCl NaCl NaCl C 800 ul + 400 ul 400 ul 400 ul400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul control NaClNaCl NaCl NaCl NaCl NaCl NaCl NaCl NaCl NaCl NaCl D 800 ul 400 ul 400 ul400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul compound1 NaCl NaCl NaCl NaCl NaCl NaCl NaCl NaCl NaCl NaCl NaCl E 800 ul 400 ul400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ulcompound 2 NaCl NaCl NaCl NaCl NaCl NaCl NaCl NaCl NaCl NaCl NaCl F 800ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul400 ul compound 3 NaCl NaCl NaCl NaCl NaCl NaCl NaCl NaCl NaCl NaCl NaClG 800 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul400 ul 400 ul compound 4 NaCl NaCl NaCl NaCl NaCl NaCl NaCl NaCl NaClNaCl NaCl H 800 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400 ul 400ul 400 ul 400 ul 400 ul compound 5 NaCl NaCl NaCl NaCl NaCl NaCl NaClNaCl NaCl NaCl NaCl 1 2 3 4 5 6 7 8 9 10 11 A Media Media Media MediaMedia Media Media Media Media Media Media Bla

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B Pos Pos Pos Pos Pos Pos Pos Pos Pos Pos Pos C 0.10 0.05 0.025 0.01250.00625 0.003125 0.001563 0.000781 0.000391 0.000195 9.77E−05 D 0.100.05 0.025 0.0125 0.00625 0.003125 0.001563 0.000781 0.000391 0.0001959.77E−05 E 0.10 0.05 0.025 0.0125 0.00625 0.003125 0.001563 0.0007810.000391 0.000195 9.77E−05 F 0.10 0.05 0.025 0.0125 0.00625 0.0031250.001563 0.000781 0.000391 0.000195 9.77E−05 G 0.10 0.05 0.025 0.01250.00625 0.003125 0.001563 0.000781 0.000391 0.000195 9.77E−05 H 0.100.05 0.025 0.0125 0.00625 0.003125 0.001563 0.000781 0.000391 0.0001959.77E−05

indicates data missing or illegible when filed

Test Plate Preparation

In row A of a 96 deep well plate pipette 180 ul of sterile BHI with 1%Tween 80 as a negative growth control. All other wells receive 180 ul ofinoculum. From the master plate introduce 20 ul to the corresponding rowin the test plate using an 8-channel pipette. Loaded plates are placedon a plate shaker in the 37° C. incubator and incubated overnight. Thenext day read the O.D. 600 on a plate reader. The MIC is the last wellfrom the right that has no bacterial growth.

The dimensions and values disclosed herein are not to be understood asbeing strictly limited to the exact numerical values recited. Instead,unless otherwise specified, each such dimension is intended to mean boththe recited value and a functionally equivalent range surrounding thatvalue. For example, a dimension disclosed as “40 mm” is intended to mean“about 40 mm.”

It should be understood that every maximum numerical limitation giventhroughout this specification will include every lower numericallimitation, as if such lower numerical limitations were expresslywritten herein. Every minimum numerical limitation given throughout thisspecification will include every higher numerical limitation, as if suchhigher numerical limitations were expressly written herein. Everynumerical range given throughout this specification will include everynarrower numerical range that falls within such broader numerical range,as if such narrower numerical ranges were all expressly written herein.

What is claimed is:
 1. A deodorant stick comprising: a. at least about25% of a liquid triglyceride; b. at least one antimicrobial; c. aprimary structurant with a melting point of at least about 50° C.; d.less than 8% of secondary structurants having a melting point at leastabout 60° C.; e. said stick being free of an aluminum salt; and f. saidstick having a hardness from about 80 mm*10 to about 140 mm*10, asmeasured by penetration with ASTM D-1321 needle.
 2. The deodorant stickof claim 1, wherein the antimicrobial is selected from the groupconsisting of baking soda, magnesium hydroxide, hexamidine, magnesiumcarbonate, zinc carbonate, thymol, magnesium hydroxide & magnesiumcarbonate hydroxide, sodium carbonate, magnesium carbonate hydroxide,partially carbonated magnesium hydroxide, calcium carbonate, polyvinylformate, salycilic acid, niacinamide, cinnamon essential oil, cinnamonbark essential oil, cinnamic aldehyde and combinations thereof.
 3. Thedeodorant stick of claim 1, wherein the antimicrobial is a powder with awater solubility of at most about 90 g/L at 25° C.
 4. The deodorantstick of claim 1, wherein the deodorant stick is substantially free ofbaking soda.
 5. The deodorant stick of claim 1, wherein the deodorantstick is substantially free of a synthetic fragrance.
 6. The deodorantstick of any claim 1, wherein the deodorant stick is substantially freeof silicones.
 7. The deodorant stick of claim 1, wherein the deodorantstick comprises from 0% to 5% silicones.
 8. The deodorant stick of claim1, comprising at least about 35% of a liquid triglyceride.
 9. Thedeodorant stick of claim 1, wherein the antimicrobial comprises bakingsoda.
 10. The deodorant stick of claim 1, wherein the antimicrobialcomprises magnesium hydroxide.
 11. The deodorant stick of claim 1,wherein the stick comprises from about 8% to about 20% of the primarystructurant.
 12. The deodorant stick of claim 1, wherein the primarystructurant has a melting point from about 50° C. to 75° C.
 13. Thedeodorant stick of claim 1, comprising less than 5% of secondarystructurants having a melting point above 60° C.
 14. A deodorant stickcomprising: a. at least about 35% of a liquid triglyceride; b. at leastone antimicrobial; c. a primary structurant with a melting point fromabout 50° C. to about 75° C.; d. said stick being free of an aluminumsalt; and e. said stick having a hardness from about 80 mm*10 to about140 mm*10, as measured by penetration with ASTM D-1321 needle.
 15. Thedeodorant stick of claim 14, further comprising at least about 40% ofliquid triglyceride and less than 5% of secondary structurants having amelting point greater than 60° C.
 16. The deodorant stick of claim 14,wherein the deodorant stick is substantially free of baking soda.
 17. Adeodorant stick comprising: a. at least about 40% of a liquidtriglyceride; b. at least one antimicrobial; c. a primary structurantwith a melting point from about 50° C. to about 75° C.;
 18. Thedeodorant stick of claim 17, further comprising less than 5% ofsecondary structurants having a melting point of at least about 60° C.19. The deodorant stick of claim 17, said stick having a hardness fromabout 80 mm*10 to about 140 mm*10, as measured by penetration with ASTMD-1321 needle.
 20. A method of making a deodorant stick, comprising thesteps of combining deodorant components comprising at least about 40% ofa liquid triglyceride and an antimicrobial in an open tank system,mixing the components, heating the components, and cooling thecomponents.